CN110483532B - Method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves - Google Patents
Method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves Download PDFInfo
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- CN110483532B CN110483532B CN201910838715.7A CN201910838715A CN110483532B CN 110483532 B CN110483532 B CN 110483532B CN 201910838715 A CN201910838715 A CN 201910838715A CN 110483532 B CN110483532 B CN 110483532B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention discloses a method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves, which comprises the following steps: obtaining fresh pepper leaves, and grinding into slurry; filtering the slurry to respectively obtain a first filtrate and a first filter residue; adding ethanol into the first filter residue, filtering to obtain a second filtrate and a second filter residue respectively, and mixing the first filtrate and the second filtrate to obtain a mixed filtrate: adsorbing chlorophyll in the mixed filtrate by using an adsorption column, wherein the mixed filtrate after adsorption by the adsorption column is pepper leaf juice, and eluting the adsorption column to extract the chlorophyll; distilling the pepper leaf juice to obtain an oil-water mixture; storing the oil-water mixture in a sealed pool, and uniformly and continuously injecting air into the sealed pool; transferring the sealed oil-water mixture into an oil-water separator, and obtaining aromatic oil under a high-speed centrifugal state; adding the mixed solution of acetone and ethanol into the second filter residue, stirring uniformly, filtering to obtain filtrate, concentrating the filtrate, and recovering acetone and ethanol to obtain chlorophyll. The invention reduces the use amount of the organic solvent.
Description
Technical Field
The invention relates to a preparation method of chlorophyll and aromatic oil, in particular to a method for extracting chlorophyll and aromatic oil from pepper leaves.
Background
The pepper is pungent in flavor and hot in nature and enters spleen and stomach meridians; has the effects of invigorating stomach, warming spleen and stomach for dispelling cold, eliminating dampness and relieving pain, killing parasites and detoxifying, relieving itching and removing fishy smell; mainly treats vomit, wind-cold-dampness arthralgia, toothache and other symptoms; zanthoxylum bungeanum belongs to Rutaceae, small arbor or shrub plant, and its dried fruit peel is one of eight major seasonings.
The pepper has the medicinal and edible values of fruits, the pepper leaves also have the performance and the taste of the pepper, the pepper leaves not only contain valuable aromatic oil components such as myrcene, terpinene and the like, but also contain health-care components such as flavone, chlorophyll and the like and traditional Chinese medicine components, have the functions of regulating immunity, protecting nerve cells, resisting inflammation, virus, mutagenesis, tumor and aging, and can be used as an important raw material for processing aromatic foods, seasonings, essences and spices; however, the pepper leaves are rapidly inactivated after being picked, and part of the effective components in the pepper leaves are damaged, such as: chlorophyll and part of aromatic oil components can be lost; at present, no processing technology suitable for the zanthoxylum bungeanum leaves exists, and the aromatic oil, the chlorophyll and other components in the zanthoxylum bungeanum leaves can be effectively utilized, so that a great amount of waste of the zanthoxylum bungeanum leaves is caused.
Disclosure of Invention
The invention aims to solve the technical problem that no processing technology suitable for pepper leaves exists at present, and the aromatic oil, the chlorophyll and other components in the pepper leaves can be effectively utilized to cause a great deal of waste of the pepper leaves.
The invention is realized by the following technical scheme:
the method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves comprises the following steps:
s1, obtaining fresh pepper leaves, cleaning, draining and grinding into serous fluid;
s2, squeezing and filtering the slurry obtained in the step S1 to respectively obtain a first filtrate and a first filter residue; adding ethanol into the first filter residue, filtering to obtain a second filtrate and a second filter residue respectively, and mixing the first filtrate and the second filtrate to obtain a mixed filtrate:
s3, filtering the mixed filtrate for 3-5 times, adsorbing chlorophyll in the mixed filtrate by using an adsorption column, eluting the adsorption column to extract chlorophyll, sealing the chlorophyll and storing the chlorophyll in a dark place, wherein the mixed filtrate after being adsorbed by the adsorption column is pepper leaf juice;
s4, distilling the pepper leaf juice to obtain an oil-water mixture;
s5, storing the oil-water mixture in a sealed pool, and uniformly and continuously injecting air into the sealed pool;
s6, transferring the sealed oil-water mixture into an oil-water separator, and obtaining aromatic oil under a high-speed centrifugation state;
and S7, adding the mixed solution of acetone and ethanol into the second filter residue, stirring uniformly, standing for 2-3 hours, filtering to obtain filtrate, concentrating the filtrate, recovering acetone and ethanol to obtain chlorophyll, sealing the chlorophyll, and storing the chlorophyll in a dark place.
The invention relates to an extraction technology which can extract aromatic oil and chlorophyll in zanthoxylum bungeanum leaves; the existing technology for extracting the plant aromatic oil or the chlorophyll needs to add a large amount of organic solvent, and the extracted plant aromatic oil or the chlorophyll has low purity, so that the health of people can be influenced when the technology is used in the fields of food, medical use and the like. The method can simultaneously extract chlorophyll and aromatic oil in the zanthoxylum bungeanum leaves under the condition of reducing the addition of the organic solvent.
According to the method, the pepper leaves are pretreated, firstly, the pepper leaves are prepared into the juice, so that the structure of the pepper leaves is damaged, and the extraction of effective components in the pepper leaves is facilitated; most of oil and chlorophyll in the pepper leaves can be separated from the leaves and mixed in pepper leaf juice, and the method can separate and purify aromatic oil and chlorophyll from the pepper leaf juice by means of adsorption, squeezing, oil-water separation and the like without adding a large amount of organic solvents; according to the invention, the chlorophyll is extracted before the aromatic oil is extracted, the extracted aromatic oil does not contain a large amount of pigments, and the quality of the aromatic oil is influenced in the aromatic oil due to unstable performance of the pigments, so that the aromatic oil prepared by the method has good quality; the slurry is extruded and filtered for many times, the content of active ingredients in the filtrate is high, the amount of used organic solvent is small when filter residue is treated, and a large amount of chlorophyll and aromatic oil is extracted under the condition of using a small amount of organic solvent. The invention effectively combines the physical extraction and chemical extraction methods, ensures the efficient extraction of chlorophyll and aromatic oil, reduces the use amount of organic solvent and saves the processing technology.
In step S7, the volume ratio of acetone to ethanol is 1:1-3, the concentration of ethanol is 98%, and the concentration of acetone is 96%. Compared with the filtrate, the filter residue has the advantages that the effective components in the filter residue are difficult to extract, and the extraction efficiency is low by adopting a physical means, so that the chlorophyll is extracted from the filter residue by adopting a mixture of ethanol and acetone, the extraction efficiency of the ethanol is lower than that of the acetone, but the ethanol is easier to separate and recover than the acetone, and the extraction efficiency of the chlorophyll in the filter residue is high by adopting a mixed solution of the acetone and the ethanol.
In step S5, the air pump is used for pumping air according to the volume of 40m3The air was pumped into the cell at a rate of/h for 2 hours. Air is introduced to facilitate oil-water separation.
And step S6, transferring the refined aromatic oil into a sealed tank, and storing at 0-10 deg.C for 1-3 days. The fragrant oil is easy to volatilize, so the fragrant oil is stored in a sealed way at low temperature, and the fragrant fragrance can be locked and the storage life of the fragrant oil can be prolonged.
And step S3, eluting the adsorption column to obtain an eluent, removing impurities from the eluent by a membrane separation technology, and concentrating to obtain chlorophyll. Chlorophyll can be damaged at high temperature, so that the method adopts a column chromatography mode to extract the chlorophyll, and the chlorophyll is prevented from being damaged; the method disclosed by the invention has the advantages that the chlorophyll is separated by means of column chromatography, the separation efficiency is high, the cost is low, the chlorophyll can be purified, and the purity of the obtained chlorophyll is high; after the chlorophyll is extracted, the chlorophyll is stored in a dark place, which is beneficial to protecting and storing the chlorophyll.
In step S7, the volume ratio of acetone to ethanol is 1:2, the concentration of ethanol is 98%, and the concentration of acetone is 96%. The usage amount of the ethanol in the invention is higher than that of the acetone, so that the organic solvent can be conveniently separated and recovered in the later period.
In step S1, the fresh pricklyash leaves are cleaned by cold water with the temperature of 5-10 ℃. The fresh Chinese prickly ash leaves are cleaned by adopting low-temperature cold water, so that the fresh Chinese prickly ash leaves are kept fresh.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves effectively combines physical extraction and chemical extraction methods, ensures high-efficiency extraction of chlorophyll and aromatic oil, and reduces the usage amount of organic solvent;
2. according to the method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves, fresh Chinese prickly ash leaves are preserved when raw materials are treated, and effective ingredients in the fresh Chinese prickly ash leaves can be locked;
3. the method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves controls the proportion and the addition of the mixed organic solvent, and is beneficial to the recovery of the organic solvent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
The method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves comprises the following steps:
s1, obtaining fresh pepper leaves, cleaning, draining and grinding into serous fluid;
s2, squeezing and filtering the slurry obtained in the step S1 to respectively obtain a first filtrate and a first filter residue; adding ethanol into the first filter residue, filtering to obtain a second filtrate and a second filter residue respectively, and mixing the first filtrate and the second filtrate to obtain a mixed filtrate:
s3, filtering the mixed filtrate for 3-5 times, adsorbing chlorophyll in the mixed filtrate by using an adsorption column, eluting the adsorption column by using the mixed filtrate which is adsorbed by the adsorption column as pepper leaf juice, obtaining eluent after eluting the adsorption column, removing impurities from the eluent by using a membrane separation technology, concentrating to obtain chlorophyll, sealing the chlorophyll, and storing in a dark place;
s4, distilling the pepper leaf juice to obtain an oil-water mixture;
s5, storing the oil-water mixture in a sealed pool, and uniformly and continuously injecting air into the sealed pool;
s6, transferring the sealed oil-water mixture into an oil-water separator, and obtaining aromatic oil under a high-speed centrifugation state;
and S7, adding the mixed solution of acetone and ethanol into the second filter residue, stirring uniformly, standing for 2-3 hours, filtering to obtain filtrate, concentrating the filtrate, recovering acetone and ethanol to obtain chlorophyll, sealing the chlorophyll, and storing the chlorophyll in a dark place.
In step S7, the volume ratio of acetone to ethanol is 1:1-3, the concentration of ethanol is 98%, and the concentration of acetone is 96%. Compared with the filtrate, the filter residue has the advantages that the effective components in the filter residue are difficult to extract, and the extraction efficiency is low by adopting a physical means, so that the chlorophyll is extracted from the filter residue by adopting a mixture of ethanol and acetone, the extraction efficiency of the ethanol is lower than that of the acetone, but the ethanol is easier to separate and recover than the acetone, and the extraction efficiency of the chlorophyll in the filter residue is high by adopting a mixed solution of the acetone and the ethanol.
In step S5, the air pump is used for pumping air according to the volume of 40m3The air was pumped into the cell at a rate of/h for 2 hours. Air is introduced to facilitate oil-water separation.
And step S6, transferring the refined aromatic oil into a sealed tank, and storing at 0-10 deg.C for 1-3 days. The fragrant oil is easy to volatilize, so the fragrant oil is stored in a sealed way at low temperature, and the fragrant fragrance can be locked and the storage life of the fragrant oil can be prolonged.
The invention relates to an extraction technology which can extract aromatic oil and chlorophyll in zanthoxylum bungeanum leaves; the existing technology for extracting the plant aromatic oil or the chlorophyll needs to add a large amount of organic solvent, and the extracted plant aromatic oil or the chlorophyll has low purity, so that the health of people can be influenced when the technology is used in the fields of food, medical use and the like. The method can simultaneously extract chlorophyll and aromatic oil in the zanthoxylum bungeanum leaves under the condition of reducing the addition of the organic solvent.
According to the method, the pepper leaves are pretreated, firstly, the pepper leaves are prepared into the juice, so that the structure of the pepper leaves is damaged, and the extraction of effective components in the pepper leaves is facilitated; most of oil and chlorophyll in the pepper leaves can be separated from the leaves and mixed in pepper leaf juice, and the method can separate and purify aromatic oil and chlorophyll from the pepper leaf juice by means of adsorption, squeezing, oil-water separation and the like without adding a large amount of organic solvents; according to the invention, the chlorophyll is extracted before the aromatic oil is extracted, the extracted aromatic oil does not contain a large amount of pigments, and the quality of the aromatic oil is influenced in the aromatic oil due to unstable performance of the pigments, so that the aromatic oil prepared by the method has good quality; the slurry is extruded and filtered for many times, the content of active ingredients in the filtrate is high, the amount of used organic solvent is small when filter residue is treated, and a large amount of chlorophyll and aromatic oil is extracted under the condition of using a small amount of organic solvent. The invention effectively combines the physical extraction and chemical extraction methods, ensures the efficient extraction of chlorophyll and aromatic oil, reduces the use amount of organic solvent and saves the processing technology.
Example 2
Based on example 1, the method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves comprises the following steps:
s1, obtaining fresh zanthoxylum bungeanum leaves, cleaning the fresh zanthoxylum bungeanum leaves by using cold water with the temperature of 5-10 ℃, draining, and grinding into serous fluid;
s2, squeezing and filtering the slurry obtained in the step S1 to respectively obtain a first filtrate and a first filter residue; adding ethanol into the first filter residue, filtering to obtain a second filtrate and a second filter residue respectively, and mixing the first filtrate and the second filtrate to obtain a mixed filtrate:
s3, filtering the mixed filtrate for 3-5 times, adsorbing chlorophyll in the mixed filtrate by using an adsorption column, eluting the adsorption column by using the mixed filtrate which is adsorbed by the adsorption column as pepper leaf juice, obtaining eluent after eluting the adsorption column, removing impurities from the eluent by using a membrane separation technology, concentrating to obtain chlorophyll, sealing the chlorophyll, and storing in a dark place;
s4, distilling the pepper leaf juice to obtain an oil-water mixture;
s5, storing the oil-water mixture in a sealed pool, and using an air pump to pump the mixture according to the volume of 40m3Continuously pumping air into the sealed pool at a speed of/h for 2 hours;
s6, transferring the sealed oil-water mixture into an oil-water separator, and obtaining aromatic oil under a high-speed centrifugation state;
s7, adding the mixed solution of acetone and ethanol into the second filter residue, stirring uniformly, standing for 2-3 hours, filtering to obtain filtrate, concentrating the filtrate, recovering acetone and ethanol to obtain chlorophyll, sealing the chlorophyll, and storing the chlorophyll in a dark place; the volume ratio of acetone to ethanol is 1:2, the concentration of ethanol is 98%, and the concentration of acetone is 96%;
chlorophyll can be damaged at high temperature, so that the method adopts an adsorption mode to extract the chlorophyll, and the chlorophyll is prevented from being damaged; the method disclosed by the invention has the advantages that the chlorophyll is separated by a column chromatography manner, the separation efficiency is high, the cost is low, and after the chlorophyll is extracted, the chlorophyll is stored in a dark place, so that the chlorophyll is protected and stored. The usage amount of the ethanol in the invention is higher than that of the acetone, so that the organic solvent can be conveniently separated and recovered in the later period. The fresh Chinese prickly ash leaves are cleaned by adopting low-temperature cold water, so that the fresh Chinese prickly ash leaves are kept fresh. The chlorophyll prepared in the step S7 and the chlorophyll prepared in the step S3 were mixed to obtain a chlorophyll finished product, the extraction rate of the chlorophyll finished product and the aromatic oil was calculated in the present invention, and the chlorophyll and the aromatic oil extracted by the conventional method were used as a control group, and the results are shown in table 1. Two different technologies are adopted for extracting chlorophyll and aromatic oil in the traditional process. The chlorophyll extraction rate is the mass ratio of chlorophyll extraction amount to pepper leaf raw material amount, and the aromatic oil extraction rate is the mass ratio of aromatic oil extraction amount to pepper leaf raw material amount. In the embodiment, the addition amount of the zanthoxylum bungeanum leaves is equal to that of the zanthoxylum bungeanum leaves in the control group.
TABLE 1 chlorophyll and aromatic oil extraction
| Detecting items | Chlorophyll finished product | Aromatic oil | Chlorophyll control group | Aromatic oil control group |
| Extraction Rate (mg/g) | 0.11 | 1.2 | 0.08 | 0.93 |
The extraction efficiency of this example was superior to that of the control group.
Example 3
Based on example 2, the performance of the fragrance oil extracted according to example 2 was tested, and the fragrance oil prepared according to the prior art was used as a control. The results are shown in Table 2.
TABLE 2 detection of aromatic oil Performance
| Detecting items | Aromatic oil | Control group |
| Transparency | Is transparent | Slight turbidity |
| Moisture content (%) | 0.03 | 0.12 |
| Lead (in pb), mg/kg | 0.33 | 0.52 |
| Purity (%) | 98.8 | 93.6 |
The quality of the aromatic oil prepared by the invention is superior to that of the aromatic oil prepared by the prior art.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (1)
1. The method for extracting chlorophyll and aromatic oil from Chinese prickly ash leaves is characterized by comprising the following steps:
s1, obtaining fresh pepper leaves, cleaning, draining and grinding into serous fluid;
s2, squeezing and filtering the slurry obtained in the step S1 to respectively obtain a first filtrate and a first filter residue; adding ethanol into the first filter residue, filtering to obtain a second filtrate and a second filter residue respectively, and mixing the first filtrate and the second filtrate to obtain a mixed filtrate:
s3, filtering the mixed filtrate for 3-5 times, adsorbing chlorophyll in the mixed filtrate by using an adsorption column, eluting the adsorption column to extract chlorophyll, sealing the chlorophyll and storing the chlorophyll in a dark place, wherein the mixed filtrate after being adsorbed by the adsorption column is pepper leaf juice;
s4, distilling the pepper leaf juice to obtain an oil-water mixture;
s5, storing the oil-water mixture in a sealed pool, and uniformly and continuously injecting air into the sealed pool;
s6, transferring the sealed oil-water mixture into an oil-water separator, and obtaining aromatic oil under a high-speed centrifugation state;
s7, adding the mixed solution of acetone and ethanol into the second filter residue, stirring uniformly, standing for 2-3 hours, filtering to obtain filtrate, concentrating the filtrate, recovering acetone and ethanol to obtain chlorophyll, sealing the chlorophyll, and storing the chlorophyll in a dark place;
in step S5, the air pump is used for pumping air according to the volume of 40m3Continuously pumping air into the sealed pool at a speed of/h for 2 hours;
after the aromatic oil is prepared in the step S6, transferring the fine aromatic oil into a sealed tank, and sealing and storing for 1-3 days at the low temperature of 0-10 ℃;
eluting the adsorption column in the step S3 to obtain an eluent, removing impurities from the eluent by a membrane separation technology, and concentrating to obtain chlorophyll;
in the step S7, the volume ratio of acetone to ethanol is 1:2, the concentration of ethanol is 98%, and the concentration of acetone is 96%;
in step S1, the fresh pricklyash leaves are cleaned by cold water with the temperature of 5-10 ℃.
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| CN114271467A (en) * | 2021-12-30 | 2022-04-05 | 广州百花香料股份有限公司 | A method for preparing gorgeous leaf extract and the prepared gorgeous leaf extract |
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| CN101234200A (en) * | 2008-03-04 | 2008-08-06 | 郭炳华 | Composition for improving and treating human body digestive system a plurality of malaise symptoms |
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